熔融制样-X射线荧光光谱法测定高碳铬铁中铬硅磷钛  

Determination of chromium,silicon,phosphorus and titanium in high-carbon ferrochrome by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：张延新 李京 刘斌 刘政鹏 ZHANG Yanxin;LI Jing;LIU Bin;LIU Zhengpeng(Testing and Detection Institute of Qingdao Special Iron and Steel Co.,Ltd.,Qingdao 266043,China)

机构地区：[1]青岛特殊钢铁有限公司试验检测所,山东青岛266043

出　　处：《冶金分析》2022年第12期77-82,共6页Metallurgical Analysis

摘　　要：熔融制样-X射线荧光光谱法测定高碳铬铁的关键点在于玻璃片的制备,需保证样品熔解完全和避免浸蚀铂黄坩埚。实验无需额外制备熔剂坩埚,采用适当比例的四硼酸锂和氧化硼铺底,样品与氢氧化锂、氧化硼、硝酸锶氧化剂混匀,再覆盖以四硼酸锂,通过设置合适的熔融程序,可得到满足分析要求的均质玻璃片。选取4个高碳铬铁标准样品、7个根据标准方法GB/T 4699定值的高碳铬铁样品、2个由高纯铁和高碳铬铁按照一定质量比混合配制的合成高碳铬铁样品共13个样品绘制校准曲线,建立了X射线荧光光谱法(XRF)测定高碳铬铁中铬、硅、磷、钛的方法。方法线性相关系数均大于0.996。将实验方法应用于高碳铬铁标准样品和实际样品分析,结果表明:对于标准样品,实验方法测定值和标准值基本一致;对于实际样品,实验方法测得结果的相对标准偏差(RSD,n=5)为0.15%~3.4%,测定值和标准方法GB/T 4699基本一致。The key to the determination of high-arbon ferrochrome by X-ray fluorescence spectrometry lies in the preparation of glass bead.It is necessary to ensure the complete melting of the sample and avoid the etching of platinum-gold crucible.There was no need to prepare additional flux crucible.The lithium tetraborate and boron oxide with appropriate proportion were used for bedding.The sample was mixed uniformly with the oxidant of lithium hydroxide,boron oxide and strontium nitrate,and then covered with lithium tetraborate.The homogeneous glass bead which could meet the determination requirements was obtained by selection of the proper melting program.Total of 13 samples,including 4 high-carbon ferrochrome certified reference materials,7 high-carbon ferrochrome samples with fixed values determined by standard method of GB/T 4699,and 2 synthetic high-carbon ferrochrome samples prepared by mixing high purity iron and high-carbon ferrochrome according to certain mass ratio,were selected to draw the calibration curve.Thus,a method for determination of chromium,silicon,phosphorus and titanium in high-carbon ferrochrome was established by X-ray fluorescence spectrometry(XRF).The linear correlation coefficients were all greater than 0.996.The proposed method was applied to the determination of certified reference materials and actual samples of high-carbon ferrochrome.The results were basically consistent with the standard values for certified reference materials.For the actual samples,the relative standard deviations(RSD,n=5)were between 0.15%and 3.4%,and the results were consistent with those obtained by the standard method of GB/T 4699.

关 键 词：X射线荧光光谱法(XRF) 高碳铬铁 熔融制样 铬 硅 磷 钛 

分 类 号：O657.34[理学—分析化学] TF033[理学—化学]